Process for the removal in a small volume of liquid samples placed in containers and device for the practical application of the process



0691- 1957 A. CALAME-LONGJEAN ET AL PROCESS FOR THE REMOVAL IN A SMALL VQLUME OF LIQUID SAMPLES PLACED IN CONTAINERS AND DEVICE FOR THE PRACT APPLICATION OF THE PROCESS Filed March 2, 1965 ICAL ' INVEN TO RS ANDRE CALAME-LONGJEAN CLAUDE PALLII HENRI GUILLET United States Patent Ofitice 3,35,565 Patented Oct. 31, 1967 3,350,565 PROCESS FOR THE REMOVAL IN A SMALL VOL- UME OF LIQUID SAMPLES PLACED IN CON- TAINERS AND DEVICE FOR THE PRACTICAL APPLICATION OF THE PROCESS Andr Calame-Longjean and Claude Palli, Les Escanaux,

Bagnols-sur-Ceze, Gard, and Henri Guillet, Aix-en- Provence, France, assignors to Commissariat a IEnergie Atomique, Paris, France Filed Mar. 2, 1965, Ser. No. 438,467 Claims priority, application France, Mar. 6, 1964,

Claims. (Cl. 250-106) ABSTRACT OF THE DISCLOSURE Small volumes of contaminated liquids in polythene containers are Supplied by "a compressed air conduit to a lead shielded enclosure where the containers and contents are frozen, then crushed and the fragments then heated, washed, conditioned and discharged from the enclosure.

The present invention relates to the removal, in a small volume, of samples of noxious solutions which are placed in containers.

The invention is more especially concerned with the removal of samples of radioactive solutions after these latter have been analyzed in a pilot plant, said samples being, for example, placed within flasks of polythene which are in turn enclosed within capped transporter tubes which are also formed of polythene, said transporter tubes being employed for transferring samples from the hot cells to the laboratories, then from the laboratories to a decontamination plant for conditioning and subsequent removal.

When the analyses to be performed have been completed, the sample flasks must be opened and their contents removed. Since the rubber plug which closes each sample flask is secured by means of an aluminium capsule which is crimped-on for reasons of safety, the flasks can be emptied only by means of a mechanical process which consists either in removing the caps, in splitting open the flasks or in an unclamping operation. It is then necessary to decontaminate the interior of the flasks which have contained a radioactive liquid, then to condition the flasks, containers and caps for subsequent removal. It is in fact essential to separate the radioactive liquids which are eliminated in the form of liquid efiiuents from the solid wastes which are stored in special drums prior to separate processing.

The main solutions which have been adopted up to the present time and which consist either in emptying after de-capping or in mechanical splitting have not proved easy to carry into practice on account of the problems involved in the design and development of simple mechanical equipment, in the dangers of contamination of the processing area as a result of the projection of radioactive liquids, in the difficulties attached to the decontamination of flasks and, finally, in the substantial volume required for the storage of solid wastes.

The primary aim of this invention is to provide a process for the removal of waste products which conforms to a wide range of practical requirements more effectively than has been possible heretofore, especially insofar as the disadvantages referred-to in the foregoing are overcome by said process.

The invention mainly consists of a process in which liquid samples and their contaminated containers are cooled, prior to breaking-down, to a temperature such that said containers are embrittled and the activated liquids present therein are frozen, the fragments resulting from the breaking-down or crushing operation being then reheated, washed, conditioned and discharged in a storage drum.

The invention also consists of a device for the practical application of the process comprising successively a compressed-air conduit for the supply of containers, an inclined ramp, a cooler through which liquid nitrogen is circulated, a crusher, a washing tank, a device for conditioning solid wastes, means for discharging solid wastes and liquid efiluents, the complete apparatus being disposed within a steel-walled, leak-tight enclosure which is lead-shielded and fittted with viewing windows, handling grabs, access doors, lock chambers, lighting means and all other known arrangements which are necessary.

The invention finally consists, aside from these main arrangements, in certain other arrangements which are preferably employed at the same time and which are to e considered separately or in conbination, viz:

said containers are formed of polythene,

said containers are brought within said cooler to a temperature of approximately C.,

said device additionally comprises, within said steelwalled enclosure, a lifting apparatus which serves for emergency operation in the event of failure in the normal supply of containers.

The main advantages which result from the application of the process and device in accordance with the invention are as follows:

ease of operation of the device which is largely static,

reduced contamination hazards, the active liquids being frozen at the time of crushing,

improvement of decontamination by elimination of internal corners of flasks which are always diflicult to clean,

small storage volume which is reduced in the of 4 to l.

A clearer understanding of the present invention will in any case be gained from the complementary description which follows below as well as from the accompanying drawings, it being understood that said description and drawings are given solely by way of indication and not in any limiting sense.

In the accompanying drawings:

FIG. 1 is a vertical section view along line a-a of FIG. 2 and showing a device in accordance with the invention,

FIG. 2 is a vertical sectional view along line bb of FIG. 1, with a fragmentary sectional view of the crusher.

As shown in these figures, the complete device in accordance with the invention is placed within a steel- Walled enclosure 1 which is in turn surrounded by a lead shield 2.

The full containers such as the container 3 are admitted at 4 at the top of the enclosure 1 and are directed by means of an inclined ramp 5 towards a cooler 6 in which they remain for a certain length of time. Liquid nitrogen which is circulated through said cooler is admitted through the tube 7 and discharged through the tube 8 and maintains as a result of the evaporation thereof a temperature of approximately -150 C, within the cooler.

After passing out of the cooler, the containers formed of polythene which has thus been embrittled are directed together with their frozen contents towards a crusher 9 provided with two series of discs such as 10 which are designed to crush all the containers and reduce them to small fragments. The discs such as the disc 10 are driven in rotation by a motor 11 through the intermediary of a driving belt 12, a flywheel 13 and a shaft 14 which passes proportion 3 through the shield 2 and the enclosure 1 in leak-tight manner by virtue of seals 15, 16 and 17.

The crushed fragments fall through a funnel 18 placed beneath the crusher 9 into a washing tank 19 in which the liquid effluents are then separated from the solid wastes. Three water-supply pipes such as the pipe 20 and acidsupply pipes such as the pipes 21 and 22 terminate within the top portion of said tank 19 and, as will be apparent, also pass through the enclosure 1 in leak-tight manner. Compressed air is injected at 23 into the bottom outlet of the tank 19 so as to complete the washing of the crushed containers by agitation. The liquid efiluents will be discharged through the pipe 24 which is fitted with a filter cock 25. The solid wastes, which are considerably reduced in volume, will be discharged through a conduit 27 by means of compressed air which is admitted through an intake 26.

There can also be disposed within the interior of the enclosure 1 a capping device 28 and a container lift 29 which will serve for emergency operation in the event of failure in the normal supply of containers at 4.

Provision can finally be made in the enclosure 1 for an access door 30 which is actuated by a jack 31, viewing windows such as the window 32, a lock chamber 33, a passageway 34 providing access to the crusher, a handling grab 35 which is mounted on a universal joint assembly 36, a device for providing ventilation through the openings 37, as well as lighting means and all other conventional arrangements which may prove necessary.

As will be readily understood, and as has in any case been brought out in the foregoing, the present invention is not limited in any sense to the example of construction or to the mode of application which have been more especially described and illustrated but is intended, on the contrary, to include within its scope all alternative forms, particularly in regard to the removal of any liquid 3, samples of a hazardous but not necessarily radioactive nature which are placed in containers.

What we claim is:

1. Process for the removal in small volume of samples of noxious liquid solutions in containers, the steps of cooling the liquid samples and their contaminated containers to a temperature at which the containers are embrittled and the liquids therein are frozen, then crushing the containers and frozen liquid samples therein and then heating, washing, conditioning and discharging the crushed fragments in a storage drum.

2. Process as described in claim 1, said containers being polythene.

3. Process as described in claim 1, said containers being cooled to a temperature of approximately C.

4. A device for carrying out the process of claim 1 comprising a compressed air conduit for the supply of containers, and inclined ramp connected to said conduit, a cooler through which liquid nitrogen is circulated receiving containers from said ramp, a crusher receiving containers from said cooler, a washing'tank receiving fragments from said crusher, means for conditioning solid wastes from said washing tank, means for discharging solid wastes and liquid effluents from said containing means, said device being disposed within a steel walled, leak tight, lead shielded enclosure and viewing windows, handling grabs, access doors, lock chambers and lighting means for said enclosure.

5. A device as described in claim 4 including lifting apparatus in said enclosure for emergency operation on failure of normal supply of containers.

No references cited.

RALPH G. NILSON, Primary Examiner.

A. B. CROFT, Assistant Examiner. 

1. PROCESS FOR THE REMOVAL IN SMALL VOLUME OF SAMPLES OF NOXIOUS LIQUID SOLUTIONS IN CONTAINERS, THE STEPS OF COOLING THE LIQUID SAMPLES AND THEIR CONTAMINATED CONTAINERS TO A TEMPERATURE AT WHICH THE CONTAINERS ARE EMBRITTLED AND THE LIQUIDS THEREIN ARE FROZEN, THEN CRUSHING THE CONTAINERS AND FROZEN LIQUID SAMPLES THEREIN AND THEN HEATING, WASHING, CONDITIONING AND DISCHARGING THE CRUSHED FRAGMENTS IN A STORAGE DRUM. 